Acetonitrile → HCID 23141667, 화합물

HRID 32160노트

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HRID 32160 반응식
[CH3:1][O:2][CH:3]1[CH2:8][CH2:7][N:6]([C:9]2[CH:14]=[CH:13][C:12]([N:15]3[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]3)=[C:11]([C:21]3[CH2:26][CH2:25][C:24]4([CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]4)[CH2:23][CH:22]=3)[CH:10]=2)[CH2:5][CH2:4]1.[CH3:32][O:33][CH2:34][CH2:35]Br.C(=O)([O-])[O-].[K+].[K+].C(#N)C>[Cl-].[Na+].O.C(OCC)(=O)C>[CH3:32][O:33][CH2:34][CH2:35][N:18]1[CH2:19][CH2:20][N:15]([C:12]2[CH:13]=[CH:14][C:9]([N:6]3[CH2:7][CH2:8][CH:3]([O:2][CH3:1])[CH2:4][CH2:5]3)=[CH:10][C:11]=2[C:21]2[CH2:26][CH2:25][C:24]3([CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]3)[CH2:23][CH:22]=2)[CH2:16][CH2:17]1

참가 물질

7

반응물 4

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 809722-Bromoethyl methyl etherHCID 231420141-[4-(4-Methoxypiperidin-1-yl)-2-spiro[5.5]undec-2-en-3-yl-phenyl]piperazine

생성물 1

HCID 23141667HCID 23141667, 화합물

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매2회HCID 57417360Sodium chloride; water용매

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온도
80 °C

실험 절차

A mixture of 1-[4-(4-methoxypiperidin-1-yl)-2-spiro[5.5]undec-2-en-3-yl-phenyl]piperazine (20 mg, 0.0472 mmol) produced in Example (39e), 2-bromoethyl methyl ether (0.0049 mL, 0.0519 mmol), potassium carbonate (11.1 mg, 0.0803 mmol) and acetonitrile (1 mL) was stirred for 5 hours at an external temperature of 80° C. Ethyl acetate and brine were added to the reaction mixture and extraction was performed three times with ethyl acetate. The separated organic layers were concentrated. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane) to give 1-(2-methoxyethyl)-4-[4-(4-methoxypiperidin-1-yl)-2-spiro[5.5]undec-2-en-3-ylphenyl]piperazine.

후처리

  1. concentrationThe separated organic layers were concentrated
  2. customThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-1e8ff9f29ad6468683b34d1fe9ea5440
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425554B2

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